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Simultaneous Determination of Six Fluoroquinolones in Chicken Manures by High Performance Liquid Chromatography with Fluorescence Detection |
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KeyWord:fluoroquinolones(FQs); solid-phase extraction-high performance liquid chromatography with fluorescence detection; livestock and poultry excrement; analytical method |
Author Name | Affiliation | LIU Bo | College of Resources and Environment, Hunan Agricultural University, Changsha 410128, China State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China | XUE Nan-dong | State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China | YANG Bing | State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China | GONG Dao-xin | College of Resources and Environment, Hunan Agricultural University, Changsha 410128, China | LI Fa-sheng | State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China | ZHANG Shi-lei | State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China | ZHOU Ling-li | State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China | MENG Lei | State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China | CHEN Xuan-yu | College of Resources and Environment, Hunan Agricultural University, Changsha 410128, China State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China | YAN Yun-zhong | State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China |
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Abstract: |
An analytical method for simultaneous determination of six fluoroquinolones(FQs) in chicken manures based on solid-phase extraction and high performance liquid chromatography with a fluorescence detection(HPLC/FLD) was developed in the current study. Samples were ultrasonically extracted in Mcllvaine-Na2EDTA buffer/acetonitrile(1∶1)(pH=2) for 15 min. The extract was cleaned by a HLB solid-phase extraction column, and then eluted with methanol solvent. The fluoroquinolones in the extract were determined by HPLC/FLD with acetonitrile/0.7% phosphate as mobile phase. In a concentration range of 0.01~1.0 mg·kg-1, R2 of calibration was greater than 0.99. The average percent recoveries ranged from 76.7% to 106.7% for six compounds in chicken manure samples at three different spiked levels(0.1, 0.5 mg·kg-1 and 1.0 mg·kg-1). The detection limits(LOD) were from 0.002 mg·kg-1 to 0.022 mg·kg-1, and limit of quantification(LOQ) from 0.006 8 mg·kg-1 to 0.074 mg·kg-1. This method was used to analyze six FQs in chicken manures collected from 5 chicken farms in Beijing. All six FQs were detected in most samples, with concentrations ranging from LOD to 1.13 mg·kg-1. |
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